Dichloromethane → Bis(2-chloroethyl)ethylamine

HRID 2202192

反応式

HRID 2202192 の反応式
S(Cl)([Cl:3])=O.[CH2:5]([N:7]([CH2:11]CO)[CH2:8][CH2:9]O)[CH3:6].C(=O)([O-])O.[Na+].Cl[CH2:20][Cl:21]>>[Cl:3][CH2:9][CH2:8][N:7]([CH2:11][CH2:20][Cl:21])[CH2:5][CH3:6]

参加物

5

反応物 4

HCID 6344DichloromethaneHCID 8769EthyldiethanolamineHCID 24386Thionyl ChlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 10848Bis(2-chloroethyl)ethylamine収率 76%

反応条件

温度
0 °C

実験手順

24 ml (330 mmol) of thionyl chloride are added dropwise to a solution of 20 g (150 mmol) of 2-[ethyl(2-hydroxyethyl)amino]ethanol in 200 ml of dichloromethane cooled beforehand to 0° C., and then the reaction medium is stirred at ambient temperature for 20 h. After the addition of a saturated aqueous solution of sodium hydrogen carbonate, the product is extracted with dichloromethane. The organic phase obtained is then washed with water, dried over magnesium sulfate, filtered and concentrated under vacuum. 19.5 g (76%) of bis(2-chloroethyl)ethylamine are obtained in the form of an oil.

後処理

  1. extractionthe product is extracted with dichloromethane
  2. customThe organic phase obtained
  3. washis then washed with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-c07b0c5aaaf34f73ad76b40fd4b5ca03
出典データセット
uspto-grants-2016_06
特許番号
US09365529B2

関連ノート

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